JPS61140517A - Astringent dentifrice - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a toothpaste containing an alkali gold monofluorophosphate IKB or a gelling agent or both. The components do not adversely affect each other and essentially do not react with the hydrated silica gel polish.

It has long been known that the astringent effects of zinc ions derived from water-soluble zinc salts enhance and improve oral hygiene. However, zinc ions can react with typical toothpaste ingredients, greatly reducing the benefits of zinc ions.

There were limits to the actual use of zinc.

Similarly, its monofluorophosphate ion has long been known to improve oral hygiene and inhibit tooth decay by releasing salts of fluoride, but water-soluble zinc compounds It is difficult to use them together with other toothpaste ingredients, as they lose too much of their effectiveness.

When water soluble zinc salts are used, it is preferred to use a nonionic gelling agent in the toothpaste ingredient, such as human'oxyethyl cellulose. but.

If an alkali metal salt of carboxymethyl cellulose is used in the presence of zinc ions, a reaction occurs that removes the zinc ions, destroying the gel state and causing phase separation.

Roberts et al., US Patent A72A446, states that the sequential reaction between zinc ions and the alkali metal salt of carboxymethyl cellulose produces visible particles.

Additionally, zinc astringent gel-type toothpastes have limitations due to the inability of zinc ions to coexist with various siliceous polishes.

Such polishing agents include silica xerogels, which have an average particle size ranging from 2 to 20 microns and generally have a surface area of at least about 30 microns.
0 m2/g m, typically about 300-370 m2
/Ji'm h or about 600-800 m2/gm, and in U.S. Pat. It has been stated that much of the theoretically available zinc is lost in the process.

Similarly, the question of coexistence may arise when water-soluble zinc salts are present with other toothpaste salt polishes, particularly with calcium salts such as dicalcium phosphate or calcium carbonate. The question will arise as to whether it is possible. In fact, it has long been believed that it is difficult to maintain high levels of effective zinc ions in such ordinary toothpastes, and that it is difficult to use water-soluble zinc ions.

Also when alkali metal salts of monofluorophosphate are used with such siliceous polishes in toothpastes containing water-soluble zinc salts. The question arises whether they can coexist.

Therefore, the amount of zinc ions to preserve the effects of the astringent properties of siliceous polishes and zinc and the tooth corrosion-resistant properties of fluoride salts, alkali metal monofluorophosphate salts or carboxymethylcellulose Until now, it has been difficult to create toothpastes containing alkali metal salts or both. especially.

It is possible to create a gel-type toothpaste that has both the astringent properties of zinc and the anti-corrosion properties of the teeth with and without fluoride salts due to the presence of various siliceous polishing agents. For the reason that ions and monofluorophosphates and carboxymethylcello-sulfur alkali metal salts cannot coexist.

Until now, I have not been able to put it into practical use to my satisfaction.

In the present invention, a precipitated amorphous silica gel made by the method described in Foig et al., UK Patent No. 2.03a303A and US Pat. No. 452a181, issued July 9, 1985, was used. In U.S. Pat. No. 4,528.181, a toothpaste containing precipitated amorphous silica gel is described, which contains two sources of fluoride, sodium fluoride and sodium monofluorophosphate, and fluoride as a source of calcium. Contains an alkali metal salt of stabilized phytin with improved retention.

°Such a precipitated amorphous silica gel material is a product of Gerase GMBH.

For example, Shiroblank 81. Available as Shiro Blank 81C and Shiro Blank 82. It is sold under the trademark Thyroid by Double R Brace Ant Company, Inc., and is not the same as the xerogel type, which is particularly well described in U.S. Patent No. 3538.230 to Padel et al. has been written. actually.

Some of the products sold by Gerase G.M.B.H. under the trademark Shiroblank were previously used. In addition, products with the Cyroid trademark are currently in use, such as Shiro Blank 81. Neither Shiro Blank 81G nor Shiro Blank 82 has ever been employed in a Cyroid 1 trademarked product. The grades of silica xerogel described in US Pat. No. 3,538,230 generally become more abrasive as their surface area increases.

It is particularly noted that the grades of silica gel used in this invention become less abrasive as their surface area increases.

From the perspective that most polishing agents, including the one described in U.S. Patent No. 3,538,230, have poor compatibility with zinc, special siliceous polishing agents tend not to have this problem. It is completely unexpected that the reaction between zinc ions and carboxymethylcellulose alkali metal salts is essentially weakened in the presence of such a special siliceous polishing agent. there were. Furthermore, with such a special siliceous polishing material and the presence of zinc ions, the alkali metal monofluorophosphate salt exists in a stable state.

The production of fluorine salts was completely unexpected.

Therefore, in accordance with the present invention, when using such special siliceous polishing materials, carboxymethyl cellulose should retain a high level of astringency of zinc ions or It has been found that when fluorophosphates are used, high rail fluoride ions are present.

An advantage of the present invention is to provide an astringent zinc ion-containing toothpaste that can effectively contain monofluorophosphate or carboxymethyl cellulose alkali metal salt gelling agents, or both.

A further advantage of the present invention is to provide an astringent gel-type toothpaste containing zinc ions which may optionally contain monofluorophosphate or carboxymethyl cellulose alkali metal salt gelling agents or both.

Further advantages of the invention will become apparent upon consideration of the following specification.

From this viewpoint, the present invention provides at least about 30% of this toothpaste.
a liquid vehicle containing from about 20% by weight to 90% by weight of water, a gelling agent from about 0.05% by weight to 5% by weight, and an average particle size of from 1 micron to 30 microns; and a) surface area 1-600 rrt2/I% b) pore volume 0.05 cm3/g to 0.5 cm3/g.

C) Pore volume equal to or less than 240 (unit: cm3)
/g) Product with surface area (in m2/i) d) Calculated diameter of pores from 1.5 nm to 2.5 nm.

and e) a polishing agent of about 10 to 50% by weight of synthetic precipitated amorphous silica gel with a water content of not more than 25% by weight; and up to about 50% by weight of zinc ions in the toothpaste Concerning astringent toothpastes containing water-soluble zinc salts up to 51%. Additionally, the toothpaste may contain an alkali metal salt of carboxymethylcellulose as a gelling agent and/or contain an alkali metal salt of monofluorophosphate in an amount to produce about 0.01% to 1% fluoride ions. It's okay.

As mentioned above, the synthetic precipitated amorphous silica gel is disclosed in UK Patent Application No. 2038303A and US Patent No. 4S2A1.
It is of the type described in 81. The special grade 9 of silica material described therein is preferably used in the practice of the present invention. Furthermore, the special grades published and described in October 1980 for the export products of Brace GMBH of Nordelstadt, Germany are particularly preferred, which are Shiroblank 81 and Shiroblank 82. and has the following notable physical and chemical properties: Shiroblank Shiroblank Average Particle Size (according to Coulter) um47 Wet Screen Residue (42um) % 0.02 0.0
2 pH (5% suspension in water) 36 Surface area CB-M knee T, ) m2/g 400
480 drying loss %
74S102 content (in combustion residue) % 969
9 refractive index 1.46
1.46 Shiroblank 81C can be used as a modified product of Shiroblank 81, and its p)I (5% suspension in water) is about 6 to 8.

The white blank 81 and the white blank 81C are particularly effective in polishing tooth surfaces. The white blank 82 has a small polishing effect, but can be used by consumers who desire such a weak effect.

Similarly, grades of the silica material may be mixed in proportions to provide suitable polishing performance. US Patent 4.52a
It is worth noting that although the invention described in No. 181 requires phytic salt, in the present invention, there is no abnormality in filling an empty aluminum toothpaste kit tube with the toothpaste even if there is no phytic sound. The synthetic precipitated amorphous silica gel contains about 10% to 50% by weight
%, typically about 10 to 40 t% by weight, is used in gel toothpastes.

Aqueous slurry of silica material (e.g., about 5aI, ~20
96 slurry) typically have a pH of about 2-9.

The dentifrice compositions of the invention preferably have a p)l (measured in a 10% aqueous slurry) of at least about 5.5°, such as about 5.5°.
~75. Part (p)1 of the toothpaste may be modified with suitable substances such as sodium hydroxide and the like.

The water-soluble zinc salt is present in the tooth brushing in an amount of about 5% by weight, preferably from about 0.01% to 3% by weight, and most preferably from 0.1% to 2% by weight. The water-soluble zinc salts of the present invention are soluble in water at least about 10% by weight, preferably at least 20% by weight. At least about 509% zinc ions are produced during the tooth brushing, preferably at least about 7504 zinc ions are produced, and most preferably at least about 1000 pP zinc ions are produced. Preferred zinc compounds include zinc sulfate, zinc chloride, zinc bromide, zinc iodide, zinc nitrate and zinc acetate. In the case of zinc chloride, 0.01% by weight produces about 50-pp of zinc ions and 0.2% by weight of zinc chloride produces about 11000 pp of zinc ions. Additionally, zinc oxide, a barely soluble (0,0005%) zinc compound, may be added to the toothpaste to prevent the pH from dropping. This compound acts as a buffer system and improves pH stability and is not affected by the negative effects of empty aluminum tubes. About o,
Zinc oxide having an amount of 0.5 to 0.5 couls may be present.

The toothpaste consists of a liquid vehicle containing about 30% to 60% water by weight, and is typically mixed with at least one humectant. The liquid phase is about 20% by weight of the toothpaste
The water in a gel toothpaste typically consists of 90% by weight and will be essentially clear in the gel toothpaste or essentially transparent except for an opacifying agent such as titanium dioxide that is present. About 3% to 50% by weight, preferably about 3%
present by weight% to 10% by weight, and about 10% to 1:chill 90%
In a translucent milky white gel toothpaste containing a moisturizer by weight, preferably from about 15 to 80 g, about 1
1% to 50% by weight of water is present. Typical humectants are glycerin, sorbitol (eg 70% solution), maltitol, polyethylene glycols with a molecular weight of about 400-600.

Includes propylene glycol and mixtures thereof.

That tooth brushing again. Contains a gelling agent or binder agent as a solid vehicle material, even if the amount is small,
The synthetic precipitated silica can have the effect of thickening or gelling the toothpaste into a cream or soft paste. In the present invention, carboxymethylcellulose alkalis are preferred, but other gelling agents include hydroxyethylcellulose, hydroxypropylcellulose, xanthocene, Eilland 9 moss, carrageenan, gum tragacanth, polyvinylpyrrolidone, starch and mixtures thereof. Alternatively, a binder may be used. Such gelling agents are present in an amount of about 0.05% to 5%, typically about 0.05% to 2%, preferably about 0.1% to 1.5% by weight. May be used. Particularly preferably, sodium carboxymethylcellulose is used.

Alkali metal salts such as sodium monofluorophosphate and potassium monofluorophosphate are present in the toothpaste. Sodium monofluorophosphate is particularly preferred.

In the past, gelling agents.

When attempting to prepare a liquid toothpaste containing toothpaste, zinc and sodium monofluorophosphate, the zinc ions and fluoride salt ions became insolubilized and were virtually lost. What I didn't get was that
When the polishing agent is defined as a synthetic precipitated amorphous silica gel, high rail fluoride ion and substantial zinc ion retention is achieved. Such high levels of fluoride ion retention are not obtained when using simple fluorides such as sodium fluoride.

Commercially available sodium monofluorophosphate.

Na 2P03F varies in its purity. The compound may be used in any suitable purity, provided that any impurities do not substantially impair its desired dentifrice properties. Generally, the purity is at least 80% by weight of sodium monofluorophosphate, preferably at least 90% by weight of the sodium monofluorophosphate, as compared to major manufacturing by-products or impurities such as sodium fluoride and water-soluble sodium phosphate salts. % by weight is preferred. If you express it in another way.

The sodium monofluorophosphate used has a total fluoride content of at least 12%, preferably 12.7%, and a free sodium fluoride content of no more than 1.5%, preferably 1.7%. The content should not exceed 2%;
The sodium monofluorophosphate then contains a total calculated amount of at least 12%; preferably at least 12.1% fluoride salt. The alkali metal monofluorophosphate salt has a concentration of about 0.01 i<1>
An amount is used that produces 1% by weight of fluoride salt. Therefore, sodium monofluorophosphate is about 0.076% to 7
．． 6%.

Preferably an amount of 0.76%, each of which is about 10
0-10000 ppl fluoride salt, preferably about 10
Corresponds to the fluoride salt of 00-. Can be used.

Any suitable surfactant or detergent may be included in the dentifrice composition. The surfactant or detergent that can coexist in such a toothpaste composition preferably has the ability to foam during cleaning, and preferably has the bactericidal performance of a special substance of the surfactant. selected to obtain. These detergents and surfactants are usually water-soluble compounds, and their structures may be anionic, nonionic, monoampholytic, or cationic. Generally, water soluble non-soap or synthetic organic detergents are preferred.

Suitable detergent materials are known.

For example, salts of water-soluble higher fatty acids and monoglyceride monosulfate detergents (eg, coconut fatty acid monoglyceride monosulfate sodium salts).

Includes higher alkyl sulfates (e.g., sodium lacryl sulfate), alkylaryl sulfates (e.g., sodium dodecylbenzene sulfate, L2-dihydroxypropane higher fatty acid ester sulfate), and the like.

Additionally, surfactants include higher aliphatic acylamide compounds whose acyl groups are substantially saturated with lower aliphatic aminocarboxylic acids having from 12 to 16 carbon atoms. The amino acid moiety is usually derived from the lower aliphatic saturated monoaminocarboxylic acid compound. Suitable compounds include fatty acid amides of glycine, sarcosine, alanine, 3-aminopropionic acid, and valine, the acyl group of which has approximately 12 to 16 carbon atoms.

The N-lauroyl, N-myristoyl and N-nolumitoyl sarcosine compounds are preferably used and have optimal efficacy.

The amide compound can be used in its free acid form or preferably its alkali metal salt, its ammonium salt,
It may be used as its water soluble salts such as its amine salts and its alkylol amine salts. Particular examples thereof are the sodium and potassium salts of N-lauroyl, myristoyl and balmitoyl sarcosine, N-lauroyl ammonium and ethanolamine of glycine and alanine. For ease of reference, 1 aminocarboxylic acid compound 11 sarcosine salt 1 and similar compounds have a free carboxyl group or a water-soluble carboxylate thereof on such compounds.

Such materials are used in pure or substantially pure form. In practice, the use of soaps and similar fatty acid substances should be avoided, as these substances tend to reduce the activity of these above-mentioned compounds. In normal practice, such higher fatty acid compounds are present at less than 15% by weight of the amide V, and preferably at less than 10% by weight of the amide material to suppress properties that impair its effectiveness.

Other particularly suitable surfactant materials are the condensates of sorbitan monostearate and approximately 20 moles of ethylene oxide, the condensates of sorbitan monostearate and ethylene oxide and propylene oxide, and the condensates of sorbitan monostearate and propylene glycol. nonionic surfactants such as condensates with (Buluronic substances) and long chain (alkyl) compounds available under the trademark Milanol C2M.
Includes amphoteric surfactants such as amide 8-alkylene-alkylated amine derivatives. Diisobutylphenoxyethoxyethyldimethylbenzylammonium chloride, benzyldimethylstearylammonium chlorite? , one aliphatic alkyl group (having 12 to 18 carbon atoms) and two (polyoxyethylene) groups attached to the nitrogen atom (typically about a total of about tertiary amines (having 2 to 50 ethanoxy repeating groups) and salts thereof, and compounds represented by the following structural formula, in which R is an aliphatic alkyl group having approximately 12 to 18 carbon atoms, and Antibacterial and bactericidal cationic surfactants, such as mineral or organic acid salts of these compounds, may also be used, where x, y and 2 are in the sum of 3 or more. Approximately 0.05 to make the toothpaste of the present invention
Preferably, from 5% to 5% by weight of the above surfactants are used.

Other materials such as IcFJ may be mixed to make the toothpaste of the present invention. To give an example of such a substance.

These include opacifying agents, preservatives, stabilizers, silicones, chlorophyll compounds and compounds made from ammonia such as urea, ammonium phosphate and mixtures thereof.

These auxiliaries are readily added to the dentifrice composition in amounts that do not essentially impair the properties and performance of the dentifrice, the appropriate auxiliary being selected and the usual amounts used.

In such cases, it may be necessary to include an antibacterial agent in the dentifrice composition of the present invention. Typical antibacterial agents may be used in an amount of about 0.01 coulometric parts to about 5% by weight of the toothpaste composition, preferably about 0.05 coulometric parts to about 1.0 parts by weight; Agents are similar to cetylpyridinium chloride and benzethonium chloride: N''-4(chlorobenzyl)-M5-(2,4-dichlorobenzyl)biguanidine;p-chlorophenylbiguanidine; 4-chloroinzhydrylbiguanidine: 4-chloro Benzhydrylguanylurea; N-3-lauroxypropyl-N5-p-ri.

lobenzyl biguanidine; L6-:)-p-chlorophenylhikuanibihexane; 1-(lauryldimethylammonium)-8-(p-
chlorobenzyldimethylammonium)-6-dichloro-2-guanidinobenzimidazole; N1p-chlorophenyl-N5, urylbiguanidine; 5-amino-L3-his(2-ethylhexyl)-5-
methylhexahydropyrimidine; and non-toxic addition salts thereof.

Any suitable flavoring agent or sweetener may be used to flavor the dentifrice compositions of the present invention.

Examples of suitable fragrance ingredients are su4amint, -! Pamint.

Includes salicylic methyl ester as well as perfumed oils such as bittergreen, sassafras, clove, saluchiano, eucalyptus, marjoram, cinnamon, lemon and orange. Suitable sweeteners are sucrose, lactose, maltose, sorbitol, cyclomene sodium, saccharin sodium, according to US Patent A938261:)
-! ! Petitvi and oxathiazine salts according to US Pat. No. 3,932,606. Suitable flavors and sweeteners may both be present at about 0.01% to 5% or more of the dentifrice composition.

The toothpaste composition can be easily filled into pressurized containers that are extruded or mixed by mechanical operation to form toothpaste creams or lined or unlined aluminum tubes or wax-lined lead tubes or plastic tubes. These are then filled into an aluminum laminate. UK patent application 2,
07Q, 695A, Published September 9, 1981 When the contents are mixed by mechanical operation, the rheological properties are very important. This dispersion machine consists of a mouthpiece for dispersion, a pulling jig, and a central rod.

The piston and manual controls are similar.

The pressurized mixing vessel may be of the aerosol or vacuum type.

Suitable pressurized mixing containers include a bag containing a collapsible product placed within a rigid container containing a propellant liquid. When such a pressurized mixing container operates the valve, the propellant liquid is separated from the toothpaste composition by a bag that does not allow the propellant liquid to pass through.

Only toothpaste comes out. This type of pressurized mixing vessel is disclosed in U.S. Pat. No. 4,828,977 and U.S. Pat.
It is described in. These Fi are called so-called Sepro mixing containers. Excel and Empyro spray containers are also used as pressurized types.

Yet another type of mixing vessel having a protective piston within the vessel is described in US Pat. No. 4.17 L757.

Such containers include a valve, a compartment containing the dentifrice composition, and a substantially propellant-impermeable protective piston (so-called It has a diamond container).

The dentifrice composition is typically prepared by premixing the liquid vehicle component and the gelling agent, and contains additives such as the monofluorophosphate and/or sweetener. The synthetic precipitated silica gel and zinc salt are mixed with the optional water and humectant. The additives used may then be added. The present invention will be illustrated by an example, which is intended to clarify an industrial example, and many modifications may not be described here. All it's are parts by weight unless otherwise indicated. Example 1 Part A B Glycerin 25.000 25.
000nlubitol (701) 47.05
0 43.830 xanthogen
0.260 0.260 Saccharin Sodium 0.170 0.170 Titanium Dioxide 1. ooo i,o
o.

Water 3.000
3.000 Zinc sulfate heptahydrate 0.
480 0.480 silica gel*
20.000 Silica xerogel**
17.000 Silica Aero Seal * *
* 6.500 Sodium hydroxide (40%) 0.280 Sodium lauryl sulfate 1.760 1.760 Fragrance 1.000 1.000 pH (20 Ti slurry) 5.9 6.1*
, used 6-lace GMB H Noshiro Blank 81; ** Used Brace GMB H Noshiroid AL1, formerly known as Siloy) 63; *** Uses thickener 244 from W.R. Grace and Company.

The theoretical value of soluble ions in each gel toothpaste is 1000pp
m or 0.100%.

Each toothpaste was time-tested at room temperature and 43°C.

Both have the commonly required softness. The measurement of available soluble zinc ions in each toothpaste is as follows: Toothpaste Composition A O,0840,0800,0500
,0910,0700,050 toothpaste composition B O,
0540,0420,0050,0490,0480,
Toothpaste composition A containing 005 Shiroblank 81 is.

It retains soluble zinc ions much better than the other common grade toothpaste composition B containing an equivalent amount of Shiroblank AL1.

White blank 81 of toothpaste composition A was changed to white blank 82.
Even if you replace it with Shiro blank 81 and Shiro blank 82
You can also replace it with a 1:1 mixture of

Similarly, very good retention of soluble zinc ions is achieved when less or no amount of IJ is used and its amount is added to sorbitol (70%).

Similarly, replace Shiro Blank 81 with Shiro Blank 81C and do not use sodium hydroxide.

Adding that amount to sorbitol (70%) also achieves very good retention of soluble zinc ions.

Instead of the same amount of sorbitol, 0.25 part of zinc oxide is mixed into each toothpaste composition A and B. This stabilizes the pH over time and improves the negative effects of long-term storage in unlined aluminum tubes.

Example 2 A milky white gel toothpaste was prepared and filled into unlined aluminum tubes as follows: Part A B Glycerin 25.000
25.000 Sorbitol (70-%)
47.050 43.550 Sodium carboxymethylcellulose 0.260 0.260
Satucalin sodium 0.170
0.170 titanium dioxide
1.000 1.000 water
3.000 3.000 Zinc sulfate heptahydrate 0.480
0.480 silica gel* 20.
000 - Silica xerogel**
17.000 Silica Aero Seal**
8 - 6.500 Sodium hydroxide (40ti) 0.280
0.280 Sodium lauryl sulfate
1.760 1.760 fragrance
1.000 1.000pH (20 Ti slurry)
5.9 6.1*. ＊＊、＊
**Same as Example 1 The theoretical value of soluble zinc ions in each gel toothpaste is 10
00 or 0. It is 100%.

Toothpaste Composition A does not require the use of thickeners to provide the required initial gel-like properties.

Each toothpaste was time tested at room temperature and 43°C. Both have the commonly required softness. The measurement of available soluble zinc ions in each toothpaste is as follows: Toothpaste Composition A O. 080 0.079 0.05
0 0.082 0.069 0.050 Toothpaste composition B O. 052 0.039 0.002 0.0
50 0.060 0.002 Toothpaste Composition A containing 0.002 Shiroblank 81 has significantly better soluble zinc compared to the other common grade dentifrice composition B containing an equivalent amount of Shiroblank 63. Retains ions. Ordinary 7 of ordinary carboxymethylcellulose sodium
Shiroblank 8 of polishing agent using MXF'' grade
There is no problem when using 1, but when Cymade 63, a polishing agent, is present, phase separation occurs and the gel-like state is destroyed.

Note that the numerical evaluations of toothpaste composition B in the 43° C. aging test after two weeks and one month reflect variations in the test in a consistent manner.

White blank 81 of toothpaste composition A was changed to white blank 82.
Even if you replace it with Shiro blank 81 and Shiro blank 82
Even if you replace it with a 1=1 mixture.

Similarly, very good retention of soluble lead ions is achieved when the amount of sorbitol (70%) is added to sorbitol (70%) with less or no use of IJium (and its respective hydroxides). .

In the same way, replace Shiro Blank 81 with Shiro Blank 81C and hydroxylate.) Do not use IJum.

Very good retention of soluble lead ions is achieved even when adding a small amount of sorbitol (70%).

When 0.25 parts of zinc oxide is mixed into each toothpaste composition A and B in place of the same amount of sorbitol, it stabilizes the pH over time and can be used in large quantities over long periods of time in unlined aluminum tubes. The negative effects of time are improved.

Example 3 A milky white gel toothpaste was prepared and filled into unlined aluminum tubes as follows: Glycerin 25.000 2
5. C) 00 sorbitol (70ti)
46.340 46.880 Sodium carboxymethyl cellulose 0.190 0.190 Sodium saccharin 0.170
0.170 titanium dioxide
1.000 1.000 water
3.000 3.000 Zinc sulfate heptahydrate 0.480 0.
480 Sodium monofluorophosphate 0.
760 −Sodium heptadide ゛
0.220 Precipitated amorphous silica gel* 20.000 20.000 Sodium hydroxide (40%) 0.300 0.
300 Sodium lauryl sulfate 1.
760 1.760 Fragrance 1.000
1.000pH (20% slurry)
6.0 5.9 *See Example 1 The theoretical value of soluble zinc ions and fluoride ions in each gel toothpaste is 11000p111 or o, i o o
%.

Each toothpaste composition was time tested at room temperature and 43°C.

The percentages of available soluble zinc ions and available soluble fluoride ions in each dentifrice composition, measured at room temperature, are shown below: Z: 1" % p % Fluoride ions as monofluorophosphate (dentifrice composition A) ; Toothpaste composition A O,66Zn 0.06
6ZnO,096F' 0.097F Toothpaste composition B O,070Zn O,0
51Zn0.100F 0.0481” Toothpaste composition A containing sodium monofluorophosphate essentially retains both zinc ions and fluoride ions compared to toothpaste composition B containing IJium. At 43° C., unlined aluminum tubes filled with dentifrice composition A were stable, while unlined aluminum tubes filled with dentifrice composition B generated gas.

When Shiroblank 81 is replaced with Xiroipiro 3 xero gel from W. R. Daleth and Cannonie, the retention of zinc ions and fluorine ions becomes lower.

Even if sodium monofluorophosphate is replaced with potassium monofluorophosphate, the measured values for toothpaste composition A yield similar results.

White blank 81 of toothpaste composition A was changed to white blank 82.
Even if you replace it with Shiro blank 81 and Shiro blank 82
You can also replace it with a 1:1 mixture of

Similarly, very good retention of soluble zinc and fluoride ions is achieved when that amount is added to sorbitol (7ou) with reduced or no use of IJium (and their respective hydroxides). .

In the same way, replace Shiro Blank 81 with Shiro Blank 81C1 and hydroxylate.) Do not use IJum.

Adding that amount to sorbitol (70%) also achieves very good retention of soluble zinc and fluoride ions.

When 0.25 parts of zinc oxide with the same amount of sorbitol was mixed with each toothpaste composition A and B, it stabilized the pH over time and when stored in unlined aluminum tubes for long periods of time. The negative effects of

Example 4 A transparent gel toothpaste was prepared and filled into unlined aluminum tubes as follows: Part A BCD Glycerin 25.00025.00025
．． 00025.000 Sorbitol (70t) 4
8.31048.59048.59048.450 Xanthogen 0.260 0.260
0.260 0.260 Satucharin Sodium
0.170 0.170 0.170 0.170 water
3.000 3.000 3
．． 000 3.000 Zinc chloride 0.
020 0.020 0.020 0.020 White Blank 81 20.000 - - 1
0.000 white blank 81G -20,0
00--White blank 82--
20.00010.000 Sodium hydroxide
0.280- - 0.140 Sodium lauryl sulfate 1.760 1.760 1.7
60 1.760 Fragrance 1.0001.000
1.0001.000 blue dye solution (1ch)
0.200 0.200 0.200 0.200Example 5 A transparent gel-like toothpaste was prepared and filled into unlined aluminum tubes as shown below: 25.0002
5.00025.00025.000nlubitol (7
0%) 48.31048.5904B, 5
9048.450 Carboxymethylcell O=sodium 0.260 0.260 0.260 0.2ω
Satucalin sodium 0.170 0.
170 0.170 0.170 water
3.000 3.000 3.000
3.000 Zinc chloride 0.0
20 o, 020 0.020 0.020 white blank 81 20.000 - -
10.000 white blank 81G
-20,000--Shiro blank 82
- - 20.00010.000 Sodium hydroxide (40%) 0.280--0.14
0 Sodium lauryl sulfate 1.760 1
．． 760 1.760 1.760 Fragrance 1
．． 000' 1.0001.0001.000 Dye solution (1%) Q, 200 0.200
0.200 0.200 Similar stability can be obtained by replacing sodium carboxymethylcellulose with potassium carboxymethylcellulose.

Example 6 A transparent gel toothpaste was prepared and filled into unlined aluminum tubes as follows: AB CD Glyceri' 25.00025.000
25,00025.000 Sorbitol (70%)
47.55047.83047.83047.690
Xanthoge 7 0.260 0.260
0.260 0.260 Satucharin Sodium
0.170 0.170 0.170 0.170 Water 3.000 3.000
3.000 3.000 Sodium monofluorophosphate 0.760 0.760 0.760 0.760 Lead chloride 0.020 0.020 0.
020 0.020 white blank 81 20.
000 - - 10.000 white blank 81
C-20,000--White blank 82
- 20.00010.000 Sodium hydroxide (40%) 0.280 --0.140 Sodium lauryl sulfate 1.760 1.760 1.760
1.760 Fragrance 1.0001.0001.
0001.000 Blue dye solution (1%) 0.2
00 0.200 0.200 0.200 Example The following translucent milky white gel toothpaste was manufactured,
Two-part AB CD Glycerin in a container that can be mixed by mechanical operation 25.000 25.000
25.000 25.000 Sorbitol (70 section)
24.970 24.870 24.870 24
J370 Iota carrageenan 0.700
0.700 0.700 0.700 Satucharin Sodium 0.170 0.170 0.17
0 0.170 water 25.
000 25.000 25.000 25.000 Zinc bromide dihydrate 0.400 -Zinc iodide o, 5oo--Zinc nitrate hexahydrate 0.500
-Zinc acetate dihydrate
0.500 white blank 81C21,0002
1,00021,00021,000 Sodium lauryl sulfate 1.760 1.760 1.760
1.760 Fragrance 1.0001.000
In the 1.0001.000 example, sodium saccharin may be replaced with sodium cyclomate.

Example 8 A translucent milky white gel toothpaste was prepared and filled into unlined aluminum tubes as follows: Glycerin 25.00025.00
025.00025.000nlubitol (70%)
24,97024.87024.87024
．． 870 carboxymethylcellulose sodium 0.7
00 0.700 0.700 0.700 Satucharin Sodium 0.170 0.170 0.
170 0.170 water
25.00025.00025.00025.00
0 Zinc bromide dihydrate 0.400-
- -Zinc iodide -0,5
00--Zinc sulfate hexahydrate--0,5
00-Zinc acetate dihydrate --
0.500 white blank 81 C21,00021,0
0021,00021,000 Sodium lauryl sulfate 1.760 1.760 1.760 1.
760 Fragrance 1.0001.0001.00
In the 01.000 example, sodium saccharin may be replaced with sodium cyclomate.

Example 9 Two-part glycerin 25.00025.0002 A translucent opalescent gel toothpaste was prepared and filled into a container that can be mixed by mechanical operation.
5.00025.000 Sorbitol (70 units)
24.21024.11024.11024.110 Iota carrageenaf 0.700 0.700
0.700 0.700 Saccharin Sodium
0.170 0.170 0.170 0.170 Water 25.00025.00
025.00025.000 Sodium monofluorophosphate 0.760 0.760 0.760 0.76
0 Zinc bromide dihydrate 0.400 - Zinc iodide - 0,500 - Zinc nitrate hexahydrate - 0,500 - Zinc acetate dihydrate
--0,500 white blank 81C
221,00021,00021,00021,000
Sodium lauryl sulfate 1.760 1.76
0 1.760 1.760 Fragrance 1.000
1.0001.0001.0 (In the Xi embodiment, sodium saccharin may be replaced with sodium 17um heptoclamate.

It will be apparent that further modifications may be made in the art as provided by the detailed description of the invention.

(5 other people)

Claims (1)

Claims: 1. about 20% to 90% by weight of a liquid vehicle containing water in an amount of at least about 3% by weight of the toothpaste; about 0.5% to 5% by weight of a gelling agent; Average particle size 1 micron ~ 30
micron and a) surface area 1 to 600 m^2/g, b) pore volume 0.05 cm^3/g to 0.5 cm^3/
g, c) Product surface area (number in m^2/g units) x pore volume (number in cm^3/g units) is 240 or less d) Calculated pore diameter is 1.5 nm to 2. 5 nm and e) a water content of not more than 25% by weight;
An astringent toothpaste containing up to about 5% water soluble zinc salts in ppm. 2. The astringent toothpaste according to claim 1, wherein the gelling agent is a carboxymethyl cellulose alkali metal salt gelling agent. 3. The astringent dentifrice of claim 1 or 2 further comprising an alkali metal monofluorophosphate salt in an amount to produce about 0.01% to 1% fluoride ions. 4. Astringent dentifrice according to any one of claims 1, 2 or 3, wherein the zinc salt is present in an amount of 0.01% to 3% by weight. 5. The zinc salt is selected from the group of zinc sulfate, zinc chloride, zinc bromide, zinc iodide, zinc nitrate, and zinc acetate. Also listed are astringent toothpastes. 6. The astringent toothpaste according to claim 5, wherein the zinc salt is zinc sulfate heptahydrate. 7. The astringent toothpaste according to claim 5, wherein the zinc salt is zinc chloride. 8. The water in the liquid vehicle accounts for about 3% by weight of the toothpaste.
2. The astringent dentifrice of claim 1, wherein the synthetic amorphous silica gel comprises about 10% to 40% by weight of the toothpaste. 9. The water in the liquid vehicle is about 11% by weight of the toothpaste.
An astringent toothpaste consisting of ~50% by weight. 10. The synthetic amorphous silica gel has the following properties: Average particle size (according to Coulter) nm a/4 b/7
c/4 wet screen residue (42um) % 0.0
2 0.02 0.02 pH (5% suspension in water) 3
6 6-8 Surface area (B.E.T.) m^2/g 7 4 7 Drying loss % 7 4 7 SiO_2 content (in combustion residue) 96 96 96 Refractive index 1.46 1.46 1.46 An astringent dentifrice according to claim 1, comprising a synthetic amorphous silica gel having at least one property of: 11. Claim 2, 4 or 5, wherein the gelling agent is carboxymethyl cellulose sodium salt
An astringent gel toothpaste as described in any of the following paragraphs. 12. Claim 3, wherein the alkali metal monofluorophosphate is sodium monofluorophosphate;
The astringent toothpaste described in either item 4 or 5. 13. The water-soluble zinc salt is present in an amount to produce about 1000 ppm of zinc ions, and the alkali metal monofluorophosphate salt is present in an amount to produce about 1000 ppm of fluorine salt. Astringent toothpaste. 14. The astringent toothpaste according to claim 13, wherein the zinc salt is zinc sulfate superhydrate and the alkali metal monofluorophosphate salt is sodium monofluorophosphate. 15. The astringent toothpaste according to any one of claims 1, 2, or 3, wherein the toothpaste is filled into an empty aluminum tube. 16. The toothpaste also contains about 0.005% to 0.5% by weight
An astringent dentifrice as claimed in any one of claims 1, 2 or 3, containing % by weight of zinc oxide.